通过式固相萃取/超高效液相色谱-串联质谱法测定鸡蛋中氯霉素、氟苯尼考和氟苯尼考胺残留
作者:
作者单位:

1.周口市疾病预防控制中心,河南 周口 466000;2.河南省疾病预防控制中心,河南 郑州 450000

作者简介:

辛晓晨 女 主管技师 研究方向为卫生理化检验 E-mail:Xin_023@163.com

通讯作者:

张二鹏 男 主管技师 研究方向为卫生理化检验 E-mail:erpengzhang@163.com

中图分类号:

R155

基金项目:

动物性食品中抗生素残留状况监测及膳食暴露风险评估研究(LHGJ20190677)


Determination of chloramphenicol, florfenicol and florfenicol amine residues in hen eggs by ultra-performance liquid chromatography-tandem mass spectrometry with pass-through solid extraction
Author:
Affiliation:

1.Center for Disease Control and Prevention of Zhoukou, He’nan Zhoukou 466000, China;2.Center for Disease Control and Prevention of He’nan, He’nan Zhengzhou 450000, China

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    摘要:

    目的 建立Captiva EMR-Lipid直通式固相萃取净化,超高效液相串联三重四级杆质谱检测鸡蛋内氯霉素类药物残留的技术。方法 样品用氨化乙腈提取,提取液经Captiva EMR-Lipid柱净化,通过电喷雾离子源,正负离子同时扫描的多反应监测模式进行检测,用内标法定量。结果 在线性范围0.03~6.0 μg/L内,3种化合物相关系数(r)皆在0.995以上,检出限氟苯尼考胺(FFA)、氟苯尼考(FF)与氯霉素(CAP)分别是0.04、0.01与0.02 μg/kg,定量限分别是0.12、0.03与0.06 μg/kg,回收率范围在92.3%~109.6%之间,相对标准偏差(n=6)范围为1.4%~8.2%。结论 此法易于操作,可实现较高准确度,适用于测定鸡蛋内FFA、FF与CAP残留。

    Abstract:

    Objective To establish a method for the determination of chloramphenicol drugs in hen eggs by ultra-performance liquid chromatography-tandem mass spectrometry with Captiva EMR-Lipid pretreatment.Methods Samples were extracted with ammoniated acetonitrile,then purified with Captiva EMR-Lipid,and finally detected by UPLC-MS/MS with electrospray ionization in multiple reaction monitoring mode via positive and negative ions scanning. Compounds were quantified by internal standard method.Results There were good linear relationships for 3 compounds in the range of 0.03-6.0 μg/L with correlation coefficients (r) not less than 0.995. The limits of detection of chloramphenicol (CAP), florfenicol (FF) and florfenicol amine (FFA) were 0.02, 0.01, 0.04 μg/kg, respectively. And the limits of quantitation were 0.06, 0.03, 0.12 μg/kg, respectively. The method recoveries were between 92.3%-109.6%,with relative standard deviations(n=6) between 1.4%-8.2%.Conclusion With simple operation and high accuracy, the method was suitable for the determination of CAP, FF and FFA in hen eggs.

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辛晓晨,卫瑾瑾,鹿尘,孙翠霞,张二鹏.通过式固相萃取/超高效液相色谱-串联质谱法测定鸡蛋中氯霉素、氟苯尼考和氟苯尼考胺残留[J].中国食品卫生杂志,2023,35(9):1297-1303.

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  • 收稿日期:2021-09-13
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  • 在线发布日期: 2024-01-12
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